CN102233067A - Method for extracting cattail pollen total flavonoids by double aqueous phases - Google Patents
Method for extracting cattail pollen total flavonoids by double aqueous phases Download PDFInfo
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- CN102233067A CN102233067A CN2011101175743A CN201110117574A CN102233067A CN 102233067 A CN102233067 A CN 102233067A CN 2011101175743 A CN2011101175743 A CN 2011101175743A CN 201110117574 A CN201110117574 A CN 201110117574A CN 102233067 A CN102233067 A CN 102233067A
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Abstract
The invention belongs to the technical field of medicaments, and relates to a method for extracting cattail pollen total flavonoids by double aqueous phases. The method is technically characterized by comprising the following steps of: performing extraction and impurity removal on a cattail pollen medicinal material to obtain crude cattail pollen extract, concentrating the crude cattail pollen extract, adding a double aqueous phase system of ethanol and phosphate, and mixing uniformly to obtain upper and lower phases; adding ethyl acetate, water and inorganic salt into the upper phase, mixing uniformly at room temperature, and performing back extraction; and taking out the ethyl acetate phase containing the cattail pollen total flavonoids, and performing reduced pressure concentration and vacuum drying on the ethyl acetate phase to obtain the cattail pollen total flavonoids. The method for extracting the cattail pollen total flavonoids from the cattail pollen by adopting the double aqueous phases is simple and feasible, can be used for continuous operation in amplified engineering, and has the advantages of high treatment quantity, low cost and no organic solvent residue.
Description
Technical field:
The invention belongs to the pharmaceutical technology field, relate to a kind of method of aqueous two-phase extraction Longbract cattail general flavone.
Background technology:
Pollen Typhae is the dry pollen of Typhaceae plant raupo Herba Typhae (Typha angustifolia L.), typha orientalis (Typha orientalis Presl.) or congener, have hemostasis, blood stasis dispelling, treating stranguria function, be used for haematemesis, metrorrhagia, traumatic hemorrhage, amenorrhea dysmenorrhea, blood strangury and dry pain.Flavones ingredient has obvious increase coronary flow, reduces effects such as heart and brain tissues oxygen consumption, blood vessel dilating, blood fat reducing and health atherosclerosis in the Pollen Typhae, and wherein main effective ingredient has typhaneoside, isorhamnetin-3-O-neohesperidin, naringenin and isorhamnetin etc.
Fu Daxu etc. are in document " HPLC of typhaneoside and isorhamnetin-3-O-neohesperidoside measures in the Longbract cattail general flavone extractive ", adopt 60% ethanol extraction, extracting solution concentrates the back and goes up macroporous resin, with water, 20% ethanol, 50% ethanol elution, the eluent vacuum drying obtains extractive of general flavone successively.In document " technical study of macroporous resin adsorption and purification Longbract cattail general flavone ", with typhaneoside and isorhamnetin-3-O-neohesperidoside content is index, studied the process conditions of absorption of HZ802 non-polar macroporous resin and purification Longbract cattail general flavone, the result shows that the HZ802 non-polar macroporous resin has the good adsorption purification performance to the total ketone of Pollen Typhae.Liu Bin etc. are with 70% ethanol extraction 3 times, and solvent load is followed successively by 8,6, and 6 times, extraction time is 60min, 60min, 30min.Chinese patent application number 03115508.1, Pollen Tyjphae extract and its production and use concentrates after adopting aquiferous ethanol (40-95%) heating extraction, centrifugal or filter, get supernatant or filtrate, use absorption with macroporous adsorbent resin, earlier remove impurity with water wash, the moisture lower alcohol eluting of reuse; Eluent is concentrated into certain volume, with ethanol (70-95%) precipitate with ethanol, goes post precipitation to be concentrated into to do or remove spray drying behind the ethanol, Pollen Tyjphae extract, and the Pollen Tyjphae extract that obtains is used to prevent and treat the myocardial ischemia cardiovascular disease.Li Weiwei etc. adopt 70% alcohol reflux, separate obtaining typhaneoside, isorhamnetin-3-O-neohesperidin, naringenin and isorhamnetin again through macroporous resin column chromatography, polyamide column chromatography and Sephadex LH-20 column chromatography.Zhang Shumin etc. adopt polyamide and silica gel column chromatography to carry out component separating in " Pollen Typhae chemical constitution study ", identify 9 flavone compounds.These methods mainly adopt conventional post chromatographic processes such as macroporous resin, silicagel column or polyamide column chromatography, have problems such as extraction ratio is low, solvent load is big, the production cycle is long, complex operation, unsuitable suitability for industrialized production.
Summary of the invention:
The objective of the invention is to overcome the technical problem that Pollen Typhae extraction process long flow path in the prior art, extraction ratio are low, be difficult to continued operation, difficult suitability for industrialized production, a kind of method of aqueous two-phase extraction Longbract cattail general flavone is provided.
The object of the present invention is achieved like this:
A kind of method of aqueous two-phase extraction Longbract cattail general flavone is characterized in that may further comprise the steps:
A. extract: cattail pollen is added methanol solution extract, obtain the Pollen Typhae crude extract behind the filtering and impurity removing;
B. aqueous two-phase extraction: get above-mentioned Pollen Typhae crude extract and concentrate the back and add ethanol and phosphate aqueous two-phase system, mixing is divided into upper and lower biphasely, will descend cooling mutually, crystallization, filtration, reclaims phosphate crystal;
C. strip: with above-mentioned addition ethyl acetate, water and the inorganic salt gone up, system chambers relaxing the bowels with purgatives of warm nature mixing is stripped, and is divided into upper and lower biphase after leaving standstill;
D. dry: get above-mentioned ethyl acetate phase, concentrating under reduced pressure, vacuum drying obtain Longbract cattail general flavone.
The ethanol mass ratio that adds among the step B is 7-25%.
Phosphate is selected the one or more combination in potassium phosphate, potassium dihydrogen phosphate or the dipotassium hydrogen phosphate for use among the step B, and the phosphate mass ratio of adding is 10-22%.
In the step B aqueous two-phase extraction, phase separation temperature is 10-25 ℃, and the phase-splitting time is 2-5 hour.
Inorganic salt is selected ammonium sulfate, magnesium sulfate, sodium chloride for use among the step C.
The phase-splitting time was 1-3 hour during step C stripped.
Advantage of the present invention is:
The method of aqueous two-phase extraction Longbract cattail general flavone of the present invention, be to utilize two aqueous phase extraction method, concentration and separation purification of flavone composition optionally, separation process is without chromatographic column, compare with traditional silica gel column chromatography, macroporous adsorbent resin column chromatography method, have that technological process is short, simple, cost is low, scalable engineering is carried out the advantage of seriality operation.
The specific embodiment:
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1:
Take by weighing the 20g Cattail Pollen, add methanol 200ml heating and refluxing extraction 2h, extract 3 times, filter, merge extractive liquid, concentrates and obtains concentrated solution 180g; Get concentrated solution and add 25g ethanol, 40gK
3PO
4With 100g water, abundant mixing was 15 ℃ of phase-splittings 4 hours; The last phase 141ml of ethanol polymer is rich in taking-up, adds water 60ml, ethyl acetate 96ml, and ammonium sulfate 3g, fully mixing left standstill phase-splitting 2 hours under the room temperature, and the taking-up ethyl acetate is carried out concentrating under reduced pressure mutually, vacuum drying obtains Longbract cattail general flavone.
Embodiment 2:
Take by weighing the 20g Cattail Pollen, add methanol 300ml heating and refluxing extraction 3h, extract 2 times, filter, merge extractive liquid, concentrates and obtains concentrated solution 195g; Get concentrated solution and add 35g ethanol, 48gK
3PO
4With 66g water, abundant mixing was 25 ℃ of phase-splittings 5 hours; The last phase 164ml of ethanol polymer is rich in taking-up, adds water 66ml, ethyl acetate 105ml, and ammonium sulfate 3g, fully mixing left standstill phase-splitting 3 hours under the room temperature, and the taking-up ethyl acetate is carried out concentrating under reduced pressure mutually, vacuum drying obtains Longbract cattail general flavone.
Embodiment 3:
Take by weighing the 30g Cattail Pollen, add methanol 240ml heating and refluxing extraction 3h, extract 3 times, filter, merge extractive liquid, concentrates and obtains concentrated solution 275g; Get concentrated solution and add 40g ethanol, 53gKH
2PO
4With 80g water, abundant mixing was 25 ℃ of phase-splittings 4 hours; The last phase 205ml of ethanol polymer is rich in taking-up, adds water 82ml, ethyl acetate 124ml, and magnesium sulfate 3g, fully mixing left standstill phase-splitting 2 hours under the room temperature, and the taking-up ethyl acetate is carried out concentrating under reduced pressure mutually, vacuum drying obtains Longbract cattail general flavone.
Embodiment 4:
Take by weighing the 30g Cattail Pollen, add methanol 360ml heating and refluxing extraction 2h, extract 2 times, filter, merge extractive liquid, concentrates and obtains concentrated solution 293g; Get concentrated solution and add 45g ethanol, 55gK
2HPO
4With 98g water, abundant mixing was 20 ℃ of phase-splittings 2 hours; The last phase 230ml of ethanol polymer is rich in taking-up, adds water 92ml, ethyl acetate 139ml, and ammonium sulfate 3g, fully mixing left standstill phase-splitting 1 hour under the room temperature, and the taking-up ethyl acetate is carried out concentrating under reduced pressure mutually, vacuum drying obtains Longbract cattail general flavone.
Embodiment 5:
Take by weighing the 50g Cattail Pollen, add methanol 400ml heating and refluxing extraction 3h, extract 2 times, filter, merge extractive liquid, concentrates and obtains concentrated solution 356g; Get concentrated solution and add 55g ethanol, 67gKH
2PO
4With 110g water, abundant mixing was 10 ℃ of phase-splittings 5 hours; The last phase 332ml of ethanol polymer is rich in taking-up, adds water 127ml, ethyl acetate 189ml, and sodium chloride 3g, fully mixing left standstill phase-splitting 3 hours under the room temperature, and the taking-up ethyl acetate is carried out concentrating under reduced pressure mutually, vacuum drying obtains Longbract cattail general flavone.
Claims (6)
1. the method for an aqueous two-phase extraction Longbract cattail general flavone is characterized in that may further comprise the steps:
A. extract: cattail pollen is added methanol solution extract, obtain the Pollen Typhae crude extract behind the filtering and impurity removing;
B. aqueous two-phase extraction: get above-mentioned Pollen Typhae crude extract and concentrate the back and add ethanol and phosphate aqueous two-phase system, mixing is divided into upper and lower biphase;
C. strip: with above-mentioned addition ethyl acetate, water and the inorganic salt gone up, system chambers relaxing the bowels with purgatives of warm nature mixing is stripped, and is divided into upper and lower biphase after leaving standstill;
D. dry: get above-mentioned ethyl acetate phase, concentrating under reduced pressure, vacuum drying obtain Longbract cattail general flavone.
2. the method for a kind of aqueous two-phase extraction Longbract cattail general flavone as claimed in claim 1 is characterized in that: the ethanol mass ratio that adds among the step B is 7-25%.
3. the method for a kind of aqueous two-phase extraction Longbract cattail general flavone as claimed in claim 1 is characterized in that: phosphate is selected the one or more combination in potassium phosphate, potassium dihydrogen phosphate or the dipotassium hydrogen phosphate for use among the step B, and the phosphate mass ratio of adding is 10-22%.
4. the method for a kind of aqueous two-phase extraction Longbract cattail general flavone as claimed in claim 1 is characterized in that: in the step B aqueous two-phase extraction, phase separation temperature is 10-25 ℃, and the phase-splitting time is 2-5 hour.
5. the method for a kind of aqueous two-phase extraction Longbract cattail general flavone as claimed in claim 1 is characterized in that: inorganic salt is selected ammonium sulfate, magnesium sulfate, sodium chloride for use among the step C.
6. the method for a kind of aqueous two-phase extraction Longbract cattail general flavone as claimed in claim 1 is characterized in that: the phase-splitting time was 1-3 hour during step C stripped.
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| CN2011101175743A CN102233067A (en) | 2011-05-06 | 2011-05-06 | Method for extracting cattail pollen total flavonoids by double aqueous phases |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN109293721A (en) * | 2018-11-28 | 2019-02-01 | 张家界普兰植物开发有限公司 | A kind of method that alcohol/salt double-aqueous phase system prepares neohesperidin in shaddock physiological fallen fruit |
-
2011
- 2011-05-06 CN CN2011101175743A patent/CN102233067A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN109293721A (en) * | 2018-11-28 | 2019-02-01 | 张家界普兰植物开发有限公司 | A kind of method that alcohol/salt double-aqueous phase system prepares neohesperidin in shaddock physiological fallen fruit |
| CN109293721B (en) * | 2018-11-28 | 2023-03-21 | 张家界普兰植物开发有限公司 | Method for preparing neohesperidin in physiological pomelo fruit drops by using alcohol/salt aqueous two-phase system |
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Application publication date: 20111109 |